+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0831 started at 13:43:56 on 11-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0831 in P2(1)/n CELL 0.71073 7.8204 19.1689 11.3839 90.000 100.727 90.000 ZERR 4.00 0.0002 0.0006 0.0003 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O FE CL UNIT 68 80 4 12 4 4 V = 1676.72 F(000) = 784.0 Mu = 1.07 mm-1 Cell Wt = 1510.56 Rho = 1.496 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 EQIV $1 x+0.5, -y+0.5, z-0.5 HTAB N1 O3_$1 HTAB O2 O1 SIZE 0.08 0.18 0.28 ACTA HTAB 2.00000 BOND $H WGHT 0.05070 1.28230 L.S. 10 TEMP -153.00 FVAR 0.58002 C1 1 0.280239 0.274961 0.402826 11.00000 0.01882 0.01692 = 0.01893 0.00177 0.00393 0.00110 C2 1 0.264050 0.235683 0.293786 11.00000 0.02318 0.02007 = 0.01760 0.00238 0.00050 0.00016 AFIX 43 H2 2 0.320614 0.246082 0.228908 11.00000 -1.20000 AFIX 0 C3 1 0.150140 0.179065 0.299024 11.00000 0.02414 0.02277 = 0.02643 -0.00090 -0.00258 -0.00246 AFIX 43 H3 2 0.116705 0.145449 0.237734 11.00000 -1.20000 AFIX 0 C4 1 0.093593 0.180402 0.410464 11.00000 0.02028 0.02217 = 0.03096 0.00484 0.00414 -0.00108 AFIX 43 H4 2 0.016892 0.147911 0.436582 11.00000 -1.20000 AFIX 0 C5 1 0.172701 0.239508 0.476812 11.00000 0.01783 0.02005 = 0.02325 0.00404 0.00567 0.00149 C6 1 0.619354 0.175824 0.518556 11.00000 0.01973 0.03129 = 0.02553 0.00570 -0.00089 0.00061 AFIX 43 H6 2 0.692899 0.215433 0.535142 11.00000 -1.20000 AFIX 0 C7 1 0.593212 0.135643 0.411893 11.00000 0.02637 0.03203 = 0.02553 0.00629 0.00958 0.01117 AFIX 43 H7 2 0.645589 0.143920 0.344293 11.00000 -1.20000 AFIX 0 C8 1 0.475593 0.081139 0.423799 11.00000 0.03494 0.02240 = 0.02933 0.00091 0.00658 0.01005 AFIX 43 H8 2 0.436077 0.046202 0.365908 11.00000 -1.20000 AFIX 0 C9 1 0.426765 0.087814 0.537831 11.00000 0.02897 0.02175 = 0.02960 0.00823 0.01010 0.00530 AFIX 43 H9 2 0.348427 0.058319 0.569064 11.00000 -1.20000 AFIX 0 C10 1 0.515592 0.146147 0.596334 11.00000 0.02595 0.02888 = 0.02037 0.00407 0.00224 0.00565 AFIX 43 H10 2 0.507495 0.162629 0.673810 11.00000 -1.20000 AFIX 0 C11 1 0.380673 0.339932 0.430236 11.00000 0.02233 0.01645 = 0.01965 0.00040 0.00550 0.00185 C12 1 0.571328 0.428102 0.365548 11.00000 0.02606 0.01565 = 0.02413 -0.00021 0.00754 -0.00130 AFIX 13 H12 2 0.589708 0.440786 0.452198 11.00000 -1.20000 AFIX 0 C13 1 0.460632 0.485565 0.296760 11.00000 0.03363 0.02072 = 0.03846 -0.00114 0.00849 0.00342 AFIX 23 H13A 2 0.515929 0.531263 0.319603 11.00000 -1.20000 H13B 2 0.344653 0.485663 0.319810 11.00000 -1.20000 AFIX 0 C14 1 0.750877 0.418590 0.333582 11.00000 0.02790 0.02379 = 0.03115 0.00134 0.01005 0.00052 AFIX 13 H14 2 0.735367 0.400021 0.250179 11.00000 -1.20000 AFIX 0 C15 1 0.848322 0.488303 0.338258 11.00000 0.03008 0.03663 = 0.04077 0.00021 0.00895 -0.01237 AFIX 137 H15A 2 0.788250 0.519182 0.275230 11.00000 -1.50000 H15B 2 0.967473 0.480031 0.326125 11.00000 -1.50000 H15C 2 0.851481 0.510221 0.416406 11.00000 -1.50000 AFIX 0 C16 1 0.856668 0.365872 0.417473 11.00000 0.03082 0.04203 = 0.05882 0.01473 0.00702 0.00964 AFIX 137 H16A 2 0.859549 0.380024 0.500541 11.00000 -1.50000 H16B 2 0.975647 0.364005 0.401834 11.00000 -1.50000 H16C 2 0.802823 0.319693 0.403979 11.00000 -1.50000 AFIX 0 C17 1 0.144098 0.252804 0.600068 11.00000 0.02538 0.02578 = 0.02850 0.00640 0.01144 0.00833 N1 3 0.475032 0.361821 0.351419 11.00000 0.02811 0.01632 = 0.02302 -0.00421 0.01103 -0.00388 AFIX 43 H1 2 0.479957 0.335679 0.288592 11.00000 -1.20000 AFIX 0 O1 4 0.373830 0.375062 0.522281 11.00000 0.03773 0.02581 = 0.02550 -0.00895 0.01618 -0.00746 O2 4 0.213284 0.308360 0.657067 11.00000 0.04119 0.03827 = 0.02548 -0.00330 0.01853 -0.00498 AFIX 147 H2A 2 0.268898 0.330811 0.613125 11.00000 -1.50000 AFIX 0 O3 4 0.054367 0.212452 0.646137 11.00000 0.03679 0.03285 = 0.03710 0.01069 0.02358 0.00369 FE1 5 0.360770 0.175629 0.438889 11.00000 0.01907 0.01511 = 0.01765 0.00121 0.00449 0.00148 CL1 6 0.433660 0.475315 0.138167 11.00000 0.05071 0.03672 = 0.03893 0.00744 -0.00538 0.00364 HKLF 4 Covalent radii and connectivity table for 2007src0831 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 FE 1.240 CL 0.990 C1 - C2 C5 C11 Fe1 C2 - C3 C1 Fe1 C3 - C2 C4 Fe1 C4 - C3 C5 Fe1 C5 - C4 C1 C17 Fe1 C6 - C7 C10 Fe1 C7 - C8 C6 Fe1 C8 - C7 C9 Fe1 C9 - C10 C8 Fe1 C10 - C9 C6 Fe1 C11 - O1 N1 C1 C12 - N1 C13 C14 C13 - C12 Cl1 C14 - C16 C12 C15 C15 - C14 C16 - C14 C17 - O3 O2 C5 N1 - C11 C12 O1 - C11 O2 - C17 O3 - C17 Fe1 - C5 C1 C9 C2 C8 C10 C7 C4 C6 C3 Cl1 - C13 Operators for generating equivalent atoms: $1 x+1/2, -y+1/2, z-1/2 22137 Reflections read, of which 370 rejected -10 =< h =< 9, -24 =< k =< 22, -14 =< l =< 14, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 10 11 -0.82 8.26 2 55.77 1 Inconsistent equivalents 3834 Unique reflections, of which 0 suppressed R(int) = 0.0629 R(sigma) = 0.0528 Friedel opposites merged Maximum memory for data reduction = 2492 / 37822 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 1 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58001 0.00110 -0.006 OSF Mean shift/esd = 0.003 Maximum = -0.029 for U11 Fe1 Max. shift = 0.000 A for H16A Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 2 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58000 0.00110 -0.007 OSF Mean shift/esd = 0.001 Maximum = -0.010 for U11 Fe1 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 3 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58001 0.00110 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Fe1 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 4 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58000 0.00110 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 Fe1 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 5 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58000 0.00110 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Fe1 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C11 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 6 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58000 0.00110 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C14 Max. dU = 0.000 for N1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 7 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58001 0.00110 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Fe1 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C16 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 8 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58001 0.00110 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for H16A Max. dU = 0.000 for C17 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 9 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58001 0.00110 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Fe1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C12 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3099 / 263469 wR2 = 0.1133 before cycle 10 for 3834 data and 211 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.58000 0.00110 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for H16B Max. dU = 0.000 for O3 Largest correlation matrix elements 0.520 U33 Fe1 / OSF 0.510 U11 Fe1 / OSF 0.506 U22 Fe1 / OSF Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.3206 0.2461 0.2289 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.1167 0.1454 0.2377 43 0.950 0.000 C3 C2 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.0169 0.1479 0.4366 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.6929 0.2154 0.5351 43 0.950 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.6456 0.1439 0.3443 43 0.950 0.000 C7 C8 C6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.4361 0.0462 0.3659 43 0.950 0.000 C8 C7 C9 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.3484 0.0583 0.5691 43 0.950 0.000 C9 C10 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.5075 0.1626 0.6738 43 0.950 0.000 C10 C9 C6 H12 0.5897 0.4408 0.4522 13 1.000 0.000 C12 N1 C13 C14 H13A 0.5159 0.5313 0.3196 23 0.990 0.000 C13 C12 Cl1 H13B 0.3447 0.4857 0.3198 23 0.990 0.000 C13 C12 Cl1 H14 0.7354 0.4000 0.2502 13 1.000 0.000 C14 C16 C12 C15 H15A 0.7882 0.5192 0.2752 137 0.980 0.000 C15 C14 H15A H15B 0.9675 0.4800 0.3261 137 0.980 0.000 C15 C14 H15A H15C 0.8515 0.5102 0.4164 137 0.980 0.000 C15 C14 H15A H16A 0.8596 0.3800 0.5005 137 0.980 0.000 C16 C14 H16A H16B 0.9756 0.3640 0.4018 137 0.980 0.000 C16 C14 H16A H16C 0.8028 0.3197 0.4040 137 0.980 0.000 C16 C14 H16A H1 0.4800 0.3357 0.2886 43 0.880 0.000 N1 C11 C12 H2A 0.2689 0.3308 0.6131 147 0.840 0.000 O2 C17 H2A 2007src0831 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.28024 0.27496 0.40283 1.00000 0.01881 0.01691 0.01893 0.00177 0.00393 0.00110 0.01816 0.00454 0.00032 0.00013 0.00022 0.00000 0.00124 0.00123 0.00119 0.00095 0.00098 0.00096 0.00051 C2 0.26405 0.23568 0.29379 1.00000 0.02318 0.02007 0.01760 0.00238 0.00051 0.00016 0.02071 0.00458 0.00033 0.00013 0.00022 0.00000 0.00129 0.00128 0.00117 0.00097 0.00101 0.00103 0.00053 H2 0.32061 0.24608 0.22891 1.00000 0.02485 0.00000 0.00000 C3 0.15014 0.17906 0.29903 1.00000 0.02414 0.02276 0.02642 -0.00090 -0.00258 -0.00246 0.02538 0.00489 0.00035 0.00014 0.00025 0.00000 0.00137 0.00139 0.00138 0.00108 0.00110 0.00110 0.00058 H3 0.11671 0.14545 0.23774 1.00000 0.03045 0.00000 0.00000 C4 0.09360 0.18040 0.41046 1.00000 0.02027 0.02217 0.03097 0.00484 0.00415 -0.00108 0.02455 0.00500 0.00034 0.00014 0.00025 0.00000 0.00129 0.00137 0.00144 0.00111 0.00110 0.00106 0.00057 H4 0.01690 0.14791 0.43658 1.00000 0.02946 0.00000 0.00000 C5 0.17270 0.23951 0.47681 1.00000 0.01783 0.02005 0.02324 0.00403 0.00566 0.00149 0.02014 0.00473 0.00032 0.00013 0.00023 0.00000 0.00120 0.00128 0.00128 0.00101 0.00102 0.00101 0.00053 C6 0.61935 0.17582 0.51856 1.00000 0.01973 0.03128 0.02553 0.00570 -0.00089 0.00061 0.02617 0.00523 0.00035 0.00015 0.00025 0.00000 0.00131 0.00154 0.00134 0.00114 0.00106 0.00112 0.00059 H6 0.69290 0.21543 0.53514 1.00000 0.03140 0.00000 0.00000 C7 0.59321 0.13564 0.41189 1.00000 0.02636 0.03202 0.02553 0.00629 0.00958 0.01116 0.02736 0.00547 0.00036 0.00015 0.00025 0.00000 0.00140 0.00155 0.00137 0.00115 0.00112 0.00118 0.00060 H7 0.64559 0.14392 0.34429 1.00000 0.03283 0.00000 0.00000 C8 0.47559 0.08114 0.42380 1.00000 0.03494 0.02240 0.02933 0.00091 0.00658 0.01005 0.02881 0.00556 0.00038 0.00015 0.00025 0.00000 0.00159 0.00143 0.00147 0.00112 0.00122 0.00120 0.00063 H8 0.43608 0.04620 0.36591 1.00000 0.03457 0.00000 0.00000 C9 0.42677 0.08781 0.53783 1.00000 0.02896 0.02174 0.02959 0.00823 0.01010 0.00530 0.02617 0.00538 0.00036 0.00014 0.00024 0.00000 0.00146 0.00138 0.00144 0.00109 0.00117 0.00112 0.00060 H9 0.34843 0.05832 0.56906 1.00000 0.03140 0.00000 0.00000 C10 0.51559 0.14615 0.59633 1.00000 0.02595 0.02888 0.02036 0.00407 0.00224 0.00565 0.02533 0.00511 0.00034 0.00015 0.00024 0.00000 0.00140 0.00147 0.00126 0.00109 0.00108 0.00115 0.00058 H10 0.50750 0.16263 0.67381 1.00000 0.03039 0.00000 0.00000 C11 0.38067 0.33993 0.43024 1.00000 0.02232 0.01644 0.01965 0.00040 0.00550 0.00186 0.01927 0.00462 0.00033 0.00013 0.00022 0.00000 0.00128 0.00124 0.00123 0.00093 0.00101 0.00098 0.00052 C12 0.57133 0.42810 0.36555 1.00000 0.02606 0.01564 0.02412 -0.00021 0.00755 -0.00130 0.02157 0.00483 0.00034 0.00013 0.00023 0.00000 0.00137 0.00126 0.00131 0.00099 0.00107 0.00105 0.00054 H12 0.58971 0.44079 0.45220 1.00000 0.02589 0.00000 0.00000 C13 0.46063 0.48557 0.29676 1.00000 0.03363 0.02072 0.03846 -0.00115 0.00849 0.00341 0.03071 0.00549 0.00039 0.00015 0.00026 0.00000 0.00159 0.00143 0.00162 0.00118 0.00128 0.00120 0.00064 H13A 0.51592 0.53126 0.31960 1.00000 0.03685 0.00000 0.00000 H13B 0.34465 0.48566 0.31981 1.00000 0.03685 0.00000 0.00000 C14 0.75088 0.41859 0.33358 1.00000 0.02789 0.02379 0.03115 0.00134 0.01005 0.00052 0.02702 0.00533 0.00036 0.00014 0.00026 0.00000 0.00148 0.00143 0.00145 0.00113 0.00117 0.00115 0.00060 H14 0.73537 0.40002 0.25018 1.00000 0.03243 0.00000 0.00000 C15 0.84832 0.48830 0.33826 1.00000 0.03008 0.03662 0.04076 0.00021 0.00895 -0.01237 0.03552 0.00550 0.00039 0.00016 0.00028 0.00000 0.00157 0.00177 0.00173 0.00133 0.00133 0.00133 0.00071 H15A 0.78825 0.51918 0.27523 1.00000 0.05328 0.00000 0.00000 H15B 0.96747 0.48003 0.32613 1.00000 0.05328 0.00000 0.00000 H15C 0.85148 0.51022 0.41640 1.00000 0.05328 0.00000 0.00000 C16 0.85667 0.36587 0.41747 1.00000 0.03082 0.04202 0.05882 0.01472 0.00702 0.00963 0.04406 0.00693 0.00041 0.00019 0.00033 0.00000 0.00166 0.00199 0.00218 0.00161 0.00155 0.00143 0.00083 H16A 0.85955 0.38003 0.50054 1.00000 0.06608 0.00000 0.00000 H16B 0.97565 0.36400 0.40183 1.00000 0.06608 0.00000 0.00000 H16C 0.80282 0.31969 0.40398 1.00000 0.06608 0.00000 0.00000 C17 0.14410 0.25280 0.60007 1.00000 0.02537 0.02578 0.02850 0.00640 0.01144 0.00833 0.02572 0.00552 0.00035 0.00014 0.00025 0.00000 0.00138 0.00147 0.00139 0.00114 0.00111 0.00115 0.00059 N1 0.47503 0.36182 0.35142 1.00000 0.02811 0.01631 0.02302 -0.00421 0.01103 -0.00388 0.02167 0.00396 0.00028 0.00011 0.00019 0.00000 0.00116 0.00109 0.00109 0.00085 0.00091 0.00090 0.00047 H1 0.47996 0.33568 0.28859 1.00000 0.02601 0.00000 0.00000 O1 0.37383 0.37506 0.52228 1.00000 0.03773 0.02581 0.02550 -0.00895 0.01618 -0.00745 0.02836 0.00343 0.00026 0.00010 0.00016 0.00000 0.00110 0.00102 0.00097 0.00079 0.00084 0.00086 0.00044 O2 0.21328 0.30836 0.65707 1.00000 0.04119 0.03826 0.02547 -0.00330 0.01853 -0.00498 0.03339 0.00385 0.00029 0.00011 0.00017 0.00000 0.00122 0.00121 0.00102 0.00088 0.00091 0.00096 0.00048 H2A 0.26889 0.33081 0.61312 1.00000 0.05009 0.00000 0.00000 O3 0.05437 0.21245 0.64614 1.00000 0.03679 0.03284 0.03710 0.01069 0.02358 0.00369 0.03343 0.00413 0.00027 0.00011 0.00018 0.00000 0.00116 0.00115 0.00114 0.00090 0.00095 0.00092 0.00049 Fe1 0.36077 0.17563 0.43889 1.00000 0.01906 0.01510 0.01765 0.00121 0.00449 0.00148 0.01713 0.00064 0.00004 0.00002 0.00003 0.00000 0.00020 0.00020 0.00019 0.00013 0.00014 0.00014 0.00012 Cl1 0.43366 0.47532 0.13817 1.00000 0.05071 0.03672 0.03893 0.00744 -0.00538 0.00364 0.04388 0.00152 0.00011 0.00004 0.00007 0.00000 0.00049 0.00045 0.00043 0.00033 0.00036 0.00037 0.00022 Final Structure Factor Calculation for 2007src0831 in P2(1)/n Total number of l.s. parameters = 211 Maximum vector length = 511 Memory required = 2888 / 25039 wR2 = 0.1133 before cycle 11 for 3834 data and 0 / 211 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0437 for 2972 Fo > 4sig(Fo) and 0.0630 for all 3834 data wR2 = 0.1133, GooF = S = 1.061, Restrained GooF = 1.061 for all data Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0203 0.0184 0.0158 C1 0.0257 0.0209 0.0155 C2 0.0344 0.0238 0.0180 C3 0.0335 0.0212 0.0189 C4 0.0262 0.0173 0.0168 C5 0.0357 0.0259 0.0169 C6 0.0428 0.0219 0.0174 C7 0.0405 0.0291 0.0168 C8 0.0381 0.0239 0.0165 C9 0.0333 0.0253 0.0174 C10 0.0233 0.0186 0.0159 C11 0.0278 0.0215 0.0155 C12 0.0388 0.0338 0.0196 C13 0.0338 0.0241 0.0232 C14 0.0461 0.0408 0.0197 C15 0.0674 0.0405 0.0243 C16 0.0392 0.0211 0.0168 C17 0.0329 0.0178 0.0143 N1 0.0468 0.0231 0.0151 O1 0.0489 0.0354 0.0159 O2 0.0551 0.0306 0.0146 O3 0.0201 0.0169 0.0145 Fe1 0.0630 0.0423 0.0264 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.028 0.042 0.058 0.076 0.097 0.123 0.155 0.213 1.000 Number in group 386. 410. 356. 383. 389. 376. 383. 383. 382. 386. GooF 0.895 1.031 1.139 1.098 1.125 1.068 1.035 0.988 0.962 1.235 K 1.076 0.962 0.925 0.952 0.970 0.988 0.997 1.010 1.026 0.983 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 384. 389. 395. 365. 389. 382. 381. 383. 381. 385. GooF 0.996 0.930 1.002 0.963 0.926 1.041 0.942 0.863 0.997 1.702 K 0.981 1.000 1.036 0.991 1.012 1.030 1.015 1.025 1.020 0.956 R1 0.169 0.130 0.100 0.085 0.061 0.055 0.044 0.033 0.030 0.040 Recommended weighting scheme: WGHT 0.0506 1.2879 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 1 1 10004.18 37587.61 13.57 1.000 5.59 1 3 2 53.36 7.56 7.17 0.014 3.49 8 1 4 -0.34 32.25 5.34 0.029 0.86 -1 0 1 7877.34 14480.38 5.11 0.621 6.97 6 0 4 2586.66 3657.49 4.38 0.312 1.09 -3 6 4 73.29 21.79 4.18 0.024 1.75 -1 8 2 89.09 28.70 4.02 0.028 2.16 2 3 1 394.57 546.17 3.91 0.121 3.03 2 6 3 167.31 99.55 3.86 0.051 1.95 -1 2 3 1554.52 1225.56 3.75 0.181 3.39 1 1 2 368.97 505.71 3.74 0.116 4.07 1 9 2 210.87 133.28 3.72 0.060 1.90 -1 7 2 6.56 32.65 3.59 0.029 2.40 0 4 0 421.50 307.13 3.36 0.090 4.79 -3 4 5 335.44 244.98 3.31 0.081 1.74 2 4 0 1701.93 1377.80 3.26 0.191 3.00 -2 4 2 496.75 638.69 3.26 0.130 2.82 0 8 4 57.90 28.17 3.22 0.027 1.82 -10 3 3 16.75 97.89 3.16 0.051 0.78 0 7 2 359.56 266.90 3.07 0.084 2.46 -1 12 2 173.39 245.09 3.06 0.081 1.52 -2 1 1 19.97 44.87 3.06 0.035 3.78 0 4 4 716.65 889.01 3.03 0.154 2.42 3 4 1 951.13 776.73 2.91 0.144 2.15 2 3 4 95.11 60.98 2.91 0.040 1.98 4 3 7 808.75 629.41 2.91 0.129 1.11 -5 0 1 846.25 667.67 2.89 0.133 1.56 -7 1 8 129.17 218.16 2.89 0.076 0.95 -1 1 5 111.80 72.52 2.87 0.044 2.25 3 0 1 4737.71 5663.89 2.81 0.388 2.40 4 6 2 231.20 170.86 2.78 0.067 1.52 0 12 1 241.66 177.81 2.76 0.069 1.58 -3 2 11 81.04 40.13 2.74 0.033 1.01 9 4 3 63.68 115.36 2.72 0.055 0.79 5 18 3 825.67 561.12 2.71 0.122 0.83 2 0 0 1759.20 2104.72 2.71 0.237 3.84 -2 9 2 503.72 403.15 2.69 0.104 1.82 4 0 6 322.88 217.14 2.69 0.076 1.23 -1 6 2 576.70 707.36 2.68 0.137 2.69 -7 10 6 -5.10 31.84 2.68 0.029 0.91 0 18 7 65.18 128.60 2.67 0.058 0.89 1 18 2 632.91 501.50 2.66 0.116 1.03 3 12 2 94.24 154.51 2.64 0.064 1.29 7 8 0 6.92 34.15 2.62 0.030 1.00 2 2 5 16.84 4.56 2.61 0.011 1.76 -1 5 6 867.07 714.93 2.59 0.138 1.70 2 10 2 39.49 12.13 2.58 0.018 1.60 -4 1 3 17.15 1.31 2.57 0.006 1.85 -2 14 8 106.71 62.91 2.56 0.041 0.98 -2 4 4 607.48 738.67 2.56 0.140 2.21 Bond lengths and angles C1 - Distance Angles C2 1.4371 (0.0035) C5 1.4636 (0.0034) 106.63 (0.21) C11 1.4745 (0.0035) 125.67 (0.22) 127.66 (0.22) Fe1 2.0235 (0.0024) 69.90 (0.14) 68.70 (0.14) 128.20 (0.18) C1 - C2 C5 C11 C2 - Distance Angles C3 1.4124 (0.0037) C1 1.4371 (0.0035) 108.72 (0.23) Fe1 2.0398 (0.0025) 70.96 (0.15) 68.68 (0.14) H2 0.9500 125.64 125.64 126.29 C2 - C3 C1 Fe1 C3 - Distance Angles C2 1.4124 (0.0037) C4 1.4193 (0.0039) 109.13 (0.23) Fe1 2.0679 (0.0026) 68.82 (0.15) 69.42 (0.15) H3 0.9500 125.43 125.43 127.94 C3 - C2 C4 Fe1 C4 - Distance Angles C3 1.4193 (0.0039) C5 1.4363 (0.0037) 108.00 (0.23) Fe1 2.0560 (0.0027) 70.32 (0.15) 68.08 (0.14) H4 0.9500 126.00 126.00 127.15 C4 - C3 C5 Fe1 C5 - Distance Angles C4 1.4363 (0.0037) C1 1.4636 (0.0034) 107.52 (0.22) C17 1.4834 (0.0037) 120.46 (0.23) 131.95 (0.24) Fe1 2.0212 (0.0025) 70.68 (0.15) 68.87 (0.14) 123.36 (0.18) C5 - C4 C1 C17 C6 - Distance Angles C7 1.4202 (0.0040) C10 1.4260 (0.0038) 107.85 (0.25) Fe1 2.0565 (0.0026) 69.43 (0.15) 69.30 (0.15) H6 0.9500 126.08 126.08 126.75 C6 - C7 C10 Fe1 C7 - Distance Angles C8 1.4151 (0.0042) C6 1.4202 (0.0040) 108.13 (0.24) Fe1 2.0480 (0.0027) 69.57 (0.15) 70.08 (0.15) H7 0.9500 125.93 125.93 125.99 C7 - C8 C6 Fe1 C8 - Distance Angles C7 1.4151 (0.0042) C9 1.4254 (0.0038) 108.06 (0.25) Fe1 2.0430 (0.0027) 69.95 (0.15) 69.35 (0.15) H8 0.9500 125.97 125.97 126.30 C8 - C7 C9 Fe1 C9 - Distance Angles C10 1.4157 (0.0040) C8 1.4254 (0.0038) 107.95 (0.24) Fe1 2.0377 (0.0026) 70.07 (0.15) 69.76 (0.15) H9 0.9500 126.03 126.03 125.72 C9 - C10 C8 Fe1 C10 - Distance Angles C9 1.4157 (0.0040) C6 1.4260 (0.0038) 108.01 (0.24) Fe1 2.0469 (0.0025) 69.37 (0.15) 70.03 (0.15) H10 0.9500 126.00 126.00 126.18 C10 - C9 C6 Fe1 C11 - Distance Angles O1 1.2551 (0.0030) N1 1.3312 (0.0032) 120.58 (0.23) C1 1.4745 (0.0035) 121.74 (0.23) 117.64 (0.22) C11 - O1 N1 C12 - Distance Angles N1 1.4704 (0.0032) C13 1.5243 (0.0037) 109.75 (0.22) C14 1.5256 (0.0038) 110.24 (0.21) 115.07 (0.22) H12 1.0000 107.14 107.14 107.14 C12 - N1 C13 C14 C13 - Distance Angles C12 1.5243 (0.0037) Cl1 1.7891 (0.0031) 112.83 (0.19) H13A 0.9900 109.02 109.02 H13B 0.9900 109.02 109.02 107.80 C13 - C12 Cl1 H13A C14 - Distance Angles C16 1.5243 (0.0041) C12 1.5256 (0.0038) 110.25 (0.24) C15 1.5343 (0.0039) 110.33 (0.25) 111.15 (0.23) H14 1.0000 108.34 108.34 108.34 C14 - C16 C12 C15 C15 - Distance Angles C14 1.5343 (0.0039) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C14 H15A H15B C16 - Distance Angles C14 1.5243 (0.0041) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C14 H16A H16B C17 - Distance Angles O3 1.2259 (0.0033) O2 1.3104 (0.0035) 121.16 (0.26) C5 1.4834 (0.0037) 119.69 (0.26) 119.14 (0.24) C17 - O3 O2 N1 - Distance Angles C11 1.3312 (0.0032) C12 1.4704 (0.0032) 122.38 (0.21) H1 0.8800 118.81 118.81 N1 - C11 C12 O1 - Distance Angles C11 1.2551 (0.0030) O1 - O2 - Distance Angles C17 1.3104 (0.0035) H2A 0.8400 109.47 O2 - C17 O3 - Distance Angles C17 1.2259 (0.0033) O3 - Fe1 - Distance Angles C5 2.0212 (0.0025) C1 2.0235 (0.0024) 42.43 (0.10) C9 2.0377 (0.0026) 120.13 (0.11) 157.93 (0.11) C2 2.0398 (0.0025) 69.89 (0.10) 41.42 (0.10) 158.66 (0.11) C8 2.0430 (0.0027) 154.65 (0.11) 160.44 (0.11) 40.89 (0.11) 122.33 (0.11) C10 2.0469 (0.0025) 108.40 (0.11) 123.26 (0.11) 40.56 (0.11) 159.17 (0.11) 68.36 (0.11) C7 2.0480 (0.0027) 163.80 (0.11) 124.97 (0.11) 68.48 (0.11) 107.18 (0.11) 40.47 (0.12) 68.36 (0.11) C4 2.0560 (0.0027) 41.24 (0.10) 69.96 (0.10) 105.62 (0.11) 68.57 (0.11) 118.42 (0.11) 124.63 (0.11) 153.83 (0.12) C6 2.0565 (0.0027) 126.84 (0.11) 109.34 (0.11) 68.32 (0.11) 122.83 (0.11) 68.11 (0.12) 40.67 (0.11) 40.49 (0.11) C3 2.0679 (0.0026) 68.79 (0.11) 68.94 (0.10) 122.37 (0.11) 40.21 (0.10) 105.25 (0.11) 159.97 (0.11) 119.90 (0.11) Fe1 - C5 C1 C9 C2 C8 C10 C7 Cl1 - Distance Angles C13 1.7891 (0.0031) Cl1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.04 2.900(3) 164.7 N1-H1...O3_$1 0.84 1.67 2.507(3) 178.2 O2-H2A...O1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)